CN102671683A - Preparation method of nanosheet self-assembled C-doped (BiO)2CO3 microsphere visible light catalyst - Google Patents
Preparation method of nanosheet self-assembled C-doped (BiO)2CO3 microsphere visible light catalyst Download PDFInfo
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- CN102671683A CN102671683A CN2012101508962A CN201210150896A CN102671683A CN 102671683 A CN102671683 A CN 102671683A CN 2012101508962 A CN2012101508962 A CN 2012101508962A CN 201210150896 A CN201210150896 A CN 201210150896A CN 102671683 A CN102671683 A CN 102671683A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 89
- 239000004005 microsphere Substances 0.000 title claims abstract description 8
- 239000003054 catalyst Substances 0.000 title abstract description 87
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 title abstract description 41
- 239000002135 nanosheet Substances 0.000 title abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 17
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000011941 photocatalyst Substances 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims abstract description 3
- KKMOSYLWYLMHAL-UHFFFAOYSA-N 2-bromo-6-nitroaniline Chemical compound NC1=C(Br)C=CC=C1[N+]([O-])=O KKMOSYLWYLMHAL-UHFFFAOYSA-N 0.000 claims description 34
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 20
- 238000001338 self-assembly Methods 0.000 claims description 16
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- QSBNOZODKXUXSP-UHFFFAOYSA-K bismuth;azane;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound N.[Bi+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QSBNOZODKXUXSP-UHFFFAOYSA-K 0.000 claims description 10
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 8
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- 239000008103 glucose Substances 0.000 claims description 8
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 6
- 229930091371 Fructose Natural products 0.000 claims description 6
- 239000005715 Fructose Substances 0.000 claims description 6
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 6
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 6
- 229930006000 Sucrose Natural products 0.000 claims description 6
- 229940072033 potash Drugs 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 235000015320 potassium carbonate Nutrition 0.000 claims description 6
- 239000005720 sucrose Substances 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 5
- 239000008107 starch Substances 0.000 claims description 5
- 235000019698 starch Nutrition 0.000 claims description 5
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 4
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 16
- 230000003197 catalytic effect Effects 0.000 abstract description 14
- 238000005406 washing Methods 0.000 abstract description 11
- 239000002244 precipitate Substances 0.000 abstract 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 24
- 230000000694 effects Effects 0.000 description 18
- 238000007146 photocatalysis Methods 0.000 description 18
- 238000006555 catalytic reaction Methods 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 14
- 239000000463 material Substances 0.000 description 13
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- 230000005540 biological transmission Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
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- 238000001228 spectrum Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 3
- 150000001621 bismuth Chemical class 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
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- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 1
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
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- 239000010937 tungsten Substances 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
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Abstract
The invention discloses a preparation method of a nanosheet self-assembled C-doped (BiO)2CO3 microsphere visible light catalyst, which comprises the following steps: (1) dissolving a bismuth-containing precursor, a soluble carbonate and a doping carbon source in a water solution, stirring for 30 minutes, transferring the obtained mixed solution into a high-pressure hydrothermal kettle, and carrying out hydrothermal reaction at 120-250 DEG C for 3-100 hours; and (2) after the hydrothermal reaction finishes, cooling, filtering out the precipitate, respectively washing the precipitate with deionized water and ethanol, and drying to obtain the nanosheet self-assembled C-doped (BiO)2CO3 microspheres. According to the C-doped (BiO)2CO3 prepared by the method disclosed by the invention, the doping C element reduces the energy gap of (BiO)2CO3, and the (BiO)2CO3 has visible light catalytic activity. The experimental result proves that the NO removal rate of the bismuthyl carbonate photocatalyst disclosed by the invention is 30-45%, which indicates that the bismuthyl carbonate photocatalyst has high visible light catalytic activity.
Description
Technical field
What the present invention relates to is a kind of nanometer sheet self assembly C doping (BiO)
2CO
3The preparation method of microsphere visible light photocatalyst.
Background technology
Environmental pollution and energy shortage are the significant challenge that current mankind faces, the attention that utilizes global environment of solar energy solution and energy problem more and more to receive Chinese scholars.Photocatalysis can directly utilize visible light degraded and mineralized water and the airborne all contaminations in the solar energy; And can low-density solar energy be converted into highdensity chemical energy and electric energy, have huge application potential at aspects such as environment purification pollutant and exploitation clean energy resourcies.
The key that photocatalysis technology moves towards environment and energy source use is to develop high-efficiency photocatalysis material.But existing catalysis material light quantum conversion efficiency is lower, the photoresponse narrow range, and the visible light utilization rate is low, and this is the subject matter of this technical development of restriction.The main path that addresses this problem has: (1) is with TiO
2For base material carries out that metal-doped, nonmetal doping, semiconductor are compound, photoactivate modification, hydrotreatment etc.; (2) development of new low-gap semiconductor material is like composite metal oxide, nitrogen oxygen metallide etc.; (3) exploitation is based on the emerging catalysis material of plasma effect, like Ag/AgX (X=Cl, Br, I) and Ag/AgI/Al
2O
3Deng.Above-mentioned three types catalysis material all shows good prospects for application in environmental contaminants degraded, photolysis water hydrogen and solar cell.
In the research to the semiconductor type photochemical catalyst, bismuth based semiconductor material has unique electronic structure, good light absorpting ability and higher photocatalysis performance, its obtain than extensive studies and exploitation.At present, the bismuth based semiconductor material that is widely used as photochemical catalyst has (BiO)
2CO
3, Bi
2WO
6, Bi
4Ti
3O
12, BiOX, BiVO
4, BiFeO
3And Bi
2Ti
2O
7, in these bismuth based semiconductor materials especially (BiO)
2CO
3Application the most extensive.At (BiO)
2CO
3Structure in, Bi 6s and Bi 6p track are participated in the formation of valence band and conduction band respectively, and energy gap is narrowed down; Bi 6s and O 2p orbital hybridization make the valence band of bismuth series photocatalyst more disperse, and help photohole moving on valence band, thereby reduce the compound of photohole and light induced electron, make the bismuth series photocatalyst have good photocatalytic activity.
Patent publication No. is that the Chinese patent document of CN101817555A discloses a kind of bismuthyl carbonate micro flowery material with graded structure and preparation method thereof; This method at first is dissolved in rare nitric acid the inside with bismuth nitrate; Then it is dropwise added in the excessive sodium carbonate liquor, obtain having the bismuthyl carbonate micro flowery material of graded structure, but the bismuthyl carbonate degree of crystallinity of this method preparation is not high; Structural instability, photocatalytic activity is not ideal enough.Patent publication No. is that the Chinese patent document of CN102275987A discloses a kind of nano-micro level plate bismuthyl carbonate material and preparation method thereof; At first prepare aqueous solution of urea; Then it is mixed with five water bismuth nitrates; Again with the mixed solution that obtains at pressure be more than the 3MPa, temperature is insulation 1 hour～4 hours under 100 ℃～200 ℃ the condition; Obtain receiving a micron plate bismuthyl carbonate material after reaction is accomplished, but the form of the bismuthyl carbonate of this method preparation is uncontrollable, makes photocatalytic activity lower.
Existing document has report (BiO)
2CO
3Undoped, energy gap are 3.1～3.5eV, can not absorb visible light, only under UV-irradiation, just have photocatalytic activity, have limited (BiO)
2CO
3The application of eka-bismuth series photocatalyst.In order to expand (BiO)
2CO
3To absorption of visible light, the present invention has adopted Hydrothermal Preparation the C that assembled by nanometer sheet mix (BiO)
2CO
3The classification microballoon.C mixes and makes (BiO)
2CO
3Energy gap reduce nano-sheet structure (BiO)
2CO
3Help the separation and the transmission of photogenerated charge in photocatalytic process, and then suppress the compound of electronics and hole, improved its photocatalysis performance; The stratiform hierarchy that is obtained by the nanometer sheet self assembly can promote the diffusion transmission of reactant and product, and light can produce reflection between nanometer sheet, and then can improve its utilization rate to light source, has further improved its photocatalysis performance.Therefore, the C doping (BiO) of the present invention's preparation
2CO
3Under radiation of visible light, show the visible light catalysis activity of enhancing.
Summary of the invention
Technical problem to be solved by this invention is that the deficiency that is directed against prior art provides a kind of nanometer sheet self assembly C doping (BiO)
2CO
3The preparation method of microsphere visible light photocatalyst.
Technical scheme of the present invention is following:
A kind of nanometer sheet self assembly C doping (BiO)
2CO
3The preparation method of microsphere visible light photocatalyst may further comprise the steps:
(1) with in bismuth-containing presoma, soluble carbon hydrochlorate and the water-soluble solution of doping carbon source, stir 30min, the gained mixed liquor is transferred to the high pressure water heating kettle, carries out hydro-thermal reaction at 120～250 ℃, and the reaction time is 3～100 hours;
(2) after hydro-thermal reaction finished, cooling leached sediment, and sediment cleans with deionized water and ethanol respectively, and oven dry promptly obtains the C doping (BiO) that is formed by the nanometer sheet self assembly
2CO
3Microballoon.
Described preparation method, the described bismuth-containing presoma of step (1) is one of bismuth citrate or bismuth citrate ammonia, the bismuth-containing precursor concentration is 0.001～1.0mol/L.
Described preparation method, said soluble carbon hydrochlorate is sodium carbonate, sodium acid carbonate, potash or saleratus.
Described preparation method, the described doping C of step (1) source is glucose, fructose, sucrose, maltose or starch.
Described preparation method, the mol ratio of said bismuth-containing presoma and said soluble carbon hydrochlorate is 1: (0.1～20).
Described preparation method, the molar ratio of said bismuth-containing presoma of step (1) and doping carbon source is 1: (0.01～1.0).
Described preparation method, 180 ℃ of the described preferred hydrothermal temperatures of step (1), the preferred reaction time is 24～48h, the mol ratio of preferred bismuth-containing presoma and doping carbon source is 1: 0.15.
Described preparation method, C mix (BiO)
2CO
3Microballoon is to be that the nanometer sheet self assembly of 10～50nm forms by thickness, and the microballoon size is 0.2～10 μ m.
Said preparation method, the compactedness when step (1) is carried out hydro-thermal reaction, promptly to account for the ratio of autoclave liner volume be 10～90% to the volume of mixed solution, preferred compactedness is 60～80%.
Described said preparation method, described nanometer sheet self assembly C doping (BiO)
2CO
3The carbon doping is 0.05～5.0% in the microballoon.
Do not mix (BiO)
2CO
3Energy gap is bigger, can not absorb visible light and not possess visible light catalysis activity.C doping (BiO) through the present invention's preparation
2CO
3, its doping C element makes (BiO)
2CO
3Energy gap reduces and has a visible light catalysis activity.C doping provided by the invention (BiO)
2CO
3Photochemical catalyst is the microballoon that nanometer sheet forms; Bismuthyl carbonate with respect to the particle form; This stratiform two-dimensional structure nanometer sheet helps separating and transmission of photoelectron and hole in light-catalysed process, and then suppresses the compound of electronics and hole, improves its photocatalysis performance; The said microballoon that is formed by the bismuthyl carbonate nanometer sheet is a hierarchy; The bismuthyl carbonate microballoon of this hierarchy can promote the diffusion transmission of reactant and product; And light can reflect between the bismuthyl carbonate nanometer sheet; Thereby improved utilization rate, further improved its photocatalysis performance light source.Bismuthyl carbonate photochemical catalyst provided by the invention has higher degree of crystallinity, and the defective of the bismuthyl carbonate of this good crystallinity is few, and then promotes separating of light induced electron and hole, further improves its photocatalysis performance.Experimental result shows that bismuthyl carbonate photochemical catalyst provided by the invention is 30%～45% to the clearance of NO, explains that it has higher visible light catalysis activity.
Description of drawings
Fig. 1 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 1 preparation;
Fig. 2 is the SEM image of the photochemical catalyst of the embodiment of the invention 1 preparation;
Fig. 3 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 2 preparations;
Fig. 4 is the SEM image of the photochemical catalyst of the embodiment of the invention 2 preparations;
Fig. 5 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 3 preparations;
Fig. 6 is the XRD figure spectrum of the photochemical catalyst of the embodiment of the invention 4 preparations;
Fig. 7 is the XRD figure spectrum of the photochemical catalyst of the embodiment of the invention 5 preparations;
Fig. 8 is the TEM image of the photochemical catalyst of the embodiment of the invention 6 preparations;
Fig. 9 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 7 preparations;
Figure 10 is the SEM image of the photochemical catalyst of the embodiment of the invention 8 preparations;
Figure 11 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 9 preparations;
Figure 12 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 10 preparations.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is elaborated.
Case study on implementation 1
0.46g sodium carbonate is dissolved in the 75mL deionized water; To wherein adding 0.0580g glucose, (mol ratio of bismuth citrate and sodium carbonate is 0.926: 1, and the mol ratio of bismuth citrate and glucose is 12.476: 1 to wherein adding the 1.6g bismuth citrate again; Bismuth citrate concentration is 0.0536mol/L); Stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 180 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
To the C doping (BiO) that obtains
2CO
3Photochemical catalyst carries out UV-vis DRS to be analyzed, and the result is as shown in Figure 1, and Fig. 1 is the C doping (BiO) of the embodiment of the invention 1 preparation
2CO
3The UV-vis DRS collection of illustrative plates of photochemical catalyst, the result shows, with do not mix (BiO)
2CO
3Compare, since the effect that C mixes, the C doping (BiO) of present embodiment preparation
2CO
3Visible light is had significantly absorption, and the broadband, forbidden band is reduced to 2.9eV.The present invention is with the C doping (BiO) that obtains
2CO
3Photochemical catalyst carries out sem analysis, and the result is as shown in Figure 2, and Fig. 2 is the SEM image of the bismuthyl carbonate photochemical catalyst of the embodiment of the invention 1 preparation, can be found out the C doping (BiO) of present embodiment preparation by Fig. 2
2CO
3The solid stratiform microballoon that photochemical catalyst forms for the nanometer sheet self assembly, diameter of micro ball are about 0.8 μ m～1.5 μ m, and nanometer sheet thickness is 40～50nm.
The present invention has studied the photocatalytic activity of the bismuthyl carbonate photochemical catalyst that obtains; Detailed process is following: in relative humidity is 60%; Oxygen content is in 21% the environment; The bismuthyl carbonate photochemical catalyst that 0.1g embodiment 1 is obtained places NO stream, and the initial concentration of said NO is 450ppb, and the flow of said NO stream is 3.3L/min; Adopt power to be 300 halogen tungsten lamps (through 400nm optical filter filter ultraviolet light) said bismuthyl carbonate photochemical catalyst is carried out radiation of visible light; The bismuth series photocatalyst that calculates embodiment 1 preparation is 36.7% to the clearance of NO, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example.The result shows, the C doping (BiO) of present embodiment 1 preparation
2CO
3Photochemical catalyst has higher visible light catalysis activity.
Case study on implementation 2
0.46g sodium carbonate is dissolved in the 75mL deionized water, and to wherein adding 0.1160g glucose, (mol ratio of bismuth citrate and sodium carbonate is 0.926: 1 to wherein adding the 1.6g bismuth citrate again; The mol ratio of bismuth citrate and glucose is 6.238: 1; Bismuth citrate concentration is 0.0536mol/L), stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 180 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
Fig. 3 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 2 preparations, and the result shows, with do not mix (BiO)
2CO
3Compare, since the effect that C mixes, the C doping (BiO) of present embodiment preparation
2CO
3Visible light is had significantly absorption, and the broadband, forbidden band is reduced to 2.7eV.The present invention is with the C doping (BiO) that obtains
2CO
3Photochemical catalyst carries out sem analysis, and the result is as shown in Figure 4, and Fig. 4 is the SEM image of the bismuthyl carbonate photochemical catalyst of the embodiment of the invention 2 preparations, can be found out the C doping (BiO) of present embodiment preparation by Fig. 4
2CO
3The solid stratiform microballoon that photochemical catalyst forms for the nanometer sheet self assembly, diameter of micro ball are about 0.8 μ m～1.2 μ m, and nanometer sheet thickness is 30～40nm.
The present invention has studied the photocatalysis performance of the photochemical catalyst of present embodiment preparation according to method that embodiment 1 provides, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example.The result shows, the C doping (BiO) of present embodiment 2 preparations
2CO
3Photochemical catalyst has higher visible light catalysis activity.
Case study on implementation 3
0.46g sodium carbonate is dissolved in the 75mL deionized water, and to wherein adding 0.20g glucose, (mol ratio of bismuth citrate and sodium carbonate is 0.926: 1 to wherein adding the 1.6g bismuth citrate again; The mol ratio of bismuth citrate and glucose is 3.618: 1; Bismuth citrate concentration is 0.0536mol/L), stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 180 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
Fig. 5 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 3 preparations, and the result shows, with do not mix (BiO)
2CO
3Compare, since the effect that C mixes, the C doping (BiO) of present embodiment preparation
2CO
3Visible light is had significantly absorption, and the broadband, forbidden band is reduced to 2.5eV.
The present invention has studied the photocatalysis performance of the photochemical catalyst of present embodiment preparation according to method that embodiment 1 provides, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example.The result shows, the C doping (BiO) of present embodiment 3 preparations
2CO
3Photochemical catalyst has higher visible light catalysis activity.
Case study on implementation 4
0.46g sodium carbonate is dissolved in the 75mL deionized water, and to wherein adding 0.1160g maltose, (mol ratio of bismuth citrate and sodium carbonate is 0.926: 1 to wherein adding the 1.6g bismuth citrate again; The mol ratio of bismuth citrate and maltose is 11.863: 1; Bismuth citrate concentration is 0.0536mol/L), stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 180 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
The C doping (BiO) of the present invention to obtaining
2CO
3Photochemical catalyst carries out the X-ray diffraction analysis, and the result is as shown in Figure 6, and Fig. 6 is the XRD figure spectrum of the bismuthyl carbonate photochemical catalyst of the embodiment of the invention 4 preparations, and the result shows, the C doping (BiO) of present embodiment preparation
2CO
3Have stable and complete (BiO)
2CO
3Crystalline structure.
The present invention has studied the photocatalysis performance of the photochemical catalyst of present embodiment preparation according to method that embodiment 1 provides, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention 4 and comparative example.The result shows, the C doping (BiO) of present embodiment preparation
2CO
3Photochemical catalyst has higher visible light catalysis activity.
Case study on implementation 5
0.60g potash is dissolved in the 75mL deionized water, and to wherein adding 0.1160g maltose, (mol ratio of bismuth citrate and potash is 0.926: 1 to wherein adding the 1.6g bismuth citrate again; The mol ratio of bismuth citrate and maltose is 11.863: 1; Bismuth citrate concentration is 0.0536mol/L), stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 180 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
The C doping (BiO) of the present invention to obtaining
2CO
3Photochemical catalyst carries out the X-ray diffraction analysis, and the result is as shown in Figure 7, and Fig. 7 is the XRD figure spectrum of the bismuthyl carbonate photochemical catalyst of the embodiment of the invention 5 preparations, and the result shows, the C doping (BiO) of present embodiment preparation
2CO
3Have stable and complete (BiO)
2CO
3Crystalline structure.
The present invention has studied the photocatalysis performance of the photochemical catalyst of present embodiment preparation according to method that embodiment 1 provides, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example.The result shows, the C doping (BiO) of present embodiment 5 preparations
2CO
3Photochemical catalyst has higher visible light catalysis activity.
Case study on implementation 6
0.60g potash is dissolved in the 75mL deionized water, and to wherein adding 0.1160g fructose, (mol ratio of bismuth citrate and potash is 0.926: 1 to wherein adding the 1.6g bismuth citrate again; The mol ratio of bismuth citrate and fructose is 6.238: 1; Bismuth citrate concentration is 0.0536mol/L), stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 180 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
The present invention is with the C doping (BiO) that obtains
2CO
3Photochemical catalyst carries out tem analysis, and the result is as shown in Figure 8, and Fig. 8 is the TEM image of the bismuthyl carbonate photochemical catalyst of the embodiment of the invention 6 preparations, can be found out the C doping (BiO) of present embodiment preparation by Fig. 6
2CO
3The microballoon that photochemical catalyst forms for the nanometer sheet self assembly, diameter of micro ball are about 1 μ m, and the center hole size is about 50nm.
The present invention has studied the photocatalysis performance of the photochemical catalyst of present embodiment preparation according to method that embodiment 1 provides, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example.The result shows, the C doping (BiO) of present embodiment 6 preparations
2CO
3Photochemical catalyst has higher visible light catalysis activity.
Case study on implementation 7
0.46g sodium carbonate is dissolved in the 75mL deionized water, and to wherein adding 0.0290g sucrose, (mol ratio of bismuth citrate and sodium carbonate is 0.926: 1 to wherein adding the 1.6g bismuth citrate again; The mol ratio of bismuth citrate and sucrose is 47.451: 1; Bismuth citrate concentration is 0.0536mol/L), stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 160 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
Fig. 9 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 7 preparations, and the result shows, with do not mix (BiO)
2CO
3Compare the C doping (BiO) of present embodiment preparation
2CO
3Visible light is had obvious absorption, and the broadband, forbidden band is reduced to 3.0eV.
The present invention has studied the photocatalysis performance of the photochemical catalyst of present embodiment preparation according to method that embodiment 1 provides, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example.The result shows, the C doping (BiO) of present embodiment 7 preparations
2CO
3Photochemical catalyst has advantages of high catalytic activity.
Case study on implementation 8
0.46g sodium carbonate is dissolved in the 75mL deionized water, and to wherein adding 0.20g starch, (mol ratio of bismuth citrate and sodium carbonate is 0.926: 1 to wherein adding the 1.6g bismuth citrate again; The mol ratio of bismuth citrate and starch can not be known (reason is that the molecular weight of starch is uncertain); Bismuth citrate concentration is 0.0536mol/L), stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 180 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
Figure 10 is the SEM image of the bismuthyl carbonate photochemical catalyst of the embodiment of the invention 8 preparations, can be found out the C doping (BiO) of present embodiment preparation by Figure 10
2CO
3The solid stratiform microballoon that photochemical catalyst forms for the nanometer sheet self assembly, diameter of micro ball are about 1 μ m～1.5 μ m, and nanometer sheet thickness is 20～30nm.
The present invention has studied the photocatalysis performance of the photochemical catalyst of present embodiment preparation according to method that embodiment 1 provides, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example.The result shows, the C doping (BiO) of present embodiment 8 preparations
2CO
3Photochemical catalyst has higher visible light catalysis activity.
Case study on implementation 9
The 0.64g sodium acid carbonate is dissolved in the 75mL deionized water, and to wherein adding 0.1160g sucrose, (mol ratio of bismuth citrate ammonia and sodium acid carbonate is 0.465: 1 to wherein adding 1.6g bismuth citrate ammonia again; The mol ratio of bismuth citrate ammonia and sucrose is 10.446: 1; Bismuth citrate ammonia concentration is 0.0472mol/L), stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 160 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
Figure 11 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 9 preparations, and the result shows, with do not mix (BiO)
2CO
3Compare the C doping (BiO) of present embodiment preparation
2CO
3Visible light is significantly absorbed apparent the absorption, and the broadband, forbidden band is reduced to 2.7eV.
The present invention has studied the photocatalysis performance of the photochemical catalyst of present embodiment preparation according to method that embodiment 1 provides, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example.The result shows, the C doping (BiO) of present embodiment 9 preparations
2CO
3Photochemical catalyst has higher visible light catalysis activity.
Case study on implementation 10
The 0.58g saleratus is dissolved in the 75mL deionized water, and to wherein adding 0.20g fructose, (mol ratio of bismuth citrate ammonia and saleratus is 0.611: 1 to wherein adding 1.6g bismuth citrate ammonia again; The mol ratio of bismuth citrate ammonia and fructose is 3.186: 1; Bismuth citrate ammonia concentration is 0.0472mol/L), stir after 30 minutes, the mixed solution that obtains is moved in the high pressure water heating kettle of 100mL, reacted 24 hours down at 210 ℃.After reaction finishes, take out product, product is centrifugal, filter, 2 washings and 2 ethanol wash, and then at 80 ℃ of solids of obtaining of oven dry down, obtain C mix (BiO)
2CO
3Photochemical catalyst.
Figure 12 is the UV-vis DRS collection of illustrative plates of the photochemical catalyst of the embodiment of the invention 10 preparations, and the result shows, with do not mix (BiO)
2CO
3Compare the C doping (BiO) of present embodiment preparation
2CO
3Visible light is significantly absorbed apparent the absorption, and the broadband, forbidden band is reduced to 2.4eV.
The present invention has studied the photocatalysis performance of the photochemical catalyst of present embodiment preparation according to method that embodiment 1 provides, and the result is as shown in table 1, the catalytic performance test result of the bismuthyl carbonate photochemical catalyst that table 1 obtains for the embodiment of the invention and comparative example.The result shows, the C doping (BiO) of present embodiment 10 preparations
2CO
3Photochemical catalyst has higher visible light catalysis activity.
The C doping (BiO) that table 1 embodiment of the invention and comparative example obtain
2CO
3The catalytic performance test result of photochemical catalyst
Can find out by table 1, under identical condition, C doping provided by the invention (BiO)
2CO
3Photochemical catalyst clearance to NO under radiation of visible light is higher than the clearance of the bismuthyl carbonate photochemical catalyst of comparative example preparation to NO, and C doping provided by the invention (BiO) is described
2CO
3Photochemical catalyst has higher visible light catalysis activity.
Should be understood that, concerning those of ordinary skills, can improve or conversion, and all these improvement and conversion all should belong to the protection domain of accompanying claims of the present invention according to above-mentioned explanation.
Claims (10)
1. a nanometer sheet self assembly C doping (BiO)
2CO
3The preparation method of microsphere visible light photocatalyst is characterized in that, may further comprise the steps:
(1) with in bismuth-containing presoma, soluble carbon hydrochlorate and the water-soluble solution of doping carbon source, stir 30min, the gained mixed liquor is transferred to the high pressure water heating kettle, carries out hydro-thermal reaction at 120～250 ℃, and the reaction time is 3～100 hours;
(2) after hydro-thermal reaction finished, cooling leached sediment, and sediment cleans with deionized water and ethanol respectively, and oven dry promptly obtains the C doping (BiO) that is formed by the nanometer sheet self assembly
2CO
3Microballoon.
2. preparation method as claimed in claim 1 is characterized in that: the described bismuth-containing presoma of step (1) is one of bismuth citrate or bismuth citrate ammonia, and the bismuth-containing precursor concentration is 0.001～1.0mol/L.
3. preparation method according to claim 3 is characterized in that, said soluble carbon hydrochlorate is sodium carbonate, sodium acid carbonate, potash or saleratus.
4. preparation method as claimed in claim 1 is characterized in that: the described doping C of step (1) source is glucose, fructose, sucrose, maltose or starch.
5. preparation method according to claim 3 is characterized in that, the mol ratio of said bismuth-containing presoma and said soluble carbon hydrochlorate is 1: (0.1～20).
6. preparation method as claimed in claim 1 is characterized in that: the molar ratio of said bismuth-containing presoma of step (1) and doping carbon source is 1: (0.01～1.0).
7. preparation method as claimed in claim 1 is characterized in that: 180 ℃ of the described preferred hydrothermal temperatures of step (1), and the preferred reaction time is 24～48h, the mol ratio of preferred bismuth-containing presoma and doping carbon source is 1: 0.15.
8. preparation method as claimed in claim 1 is characterized in that: C mix (BiO)
2CO
3Microballoon is to be that the nanometer sheet self assembly of 10～50nm forms by thickness, and the microballoon size is 0.2～10 μ m.
9. according to the said preparation method of claim 1, it is characterized in that: the compactedness when step (1) is carried out hydro-thermal reaction, promptly to account for the ratio of autoclave liner volume be 10～90% to the volume of mixed solution, preferred compactedness is 60～80%.
10. said preparation method as claimed in claim 1 is characterized in that: described nanometer sheet self assembly C doping (BiO)
2CO
3The carbon doping is 0.05～5.0% in the microballoon.
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150225 |
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| CF01 | Termination of patent right due to non-payment of annual fee |